CN102969241A - Annealing method for reducing epitaxial film defects and epitaxial film obtained by using same - Google Patents
Annealing method for reducing epitaxial film defects and epitaxial film obtained by using same Download PDFInfo
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- CN102969241A CN102969241A CN2011103405129A CN201110340512A CN102969241A CN 102969241 A CN102969241 A CN 102969241A CN 2011103405129 A CN2011103405129 A CN 2011103405129A CN 201110340512 A CN201110340512 A CN 201110340512A CN 102969241 A CN102969241 A CN 102969241A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/324—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
- H01L21/3245—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering of AIIIBV compounds
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/10—Heating of the reaction chamber or the substrate
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- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
An annealing method for reducing the defect of epitaxial film and the epitaxial film obtained by said method are characterized in that the pressure between 10MPa to 6,000MPa is applied to the epitaxial film grown on the base material by vapor deposition technique, and the epitaxial film is heated to the temperature lower than the melting point of the epitaxial film, and the pressure is applied to the epitaxial film, so the lattice stress of the epitaxial film can be further reduced, and the defect density of the epitaxial film is greatly reduced.
Description
Technical field
The epitaxial film that the present invention relates to a kind of method for annealing of epitaxial film and utilize the method to obtain relates in particular to a kind of method for annealing and epitaxial film therefrom that can effectively reduce the defective of epitaxial film.
Background technology
The epitaxy technology general reference grows up monocrystal thin films in the technique of base material, its monocrystal thin films that obtains is also referred to as epitaxial film, the employed base material of epitaxial growth is generally the monocrystal material that single crystal grain and the equal tool specific direction of atomic order are only arranged, and according to chemical composition and the lattice types difference of epitaxial film and base material, epitaxial film can be divided into homoepitaxy (Homoepitaxy) or heteroepitaxy (Heteroepitaxy), the former refers to that epitaxial film and base material are same material, are silicon or diamond such as both; Latter refers to that epitaxial film and base material are dissimilar material, such as gallium nitride (Gallium Nitride, abbreviation GaN) grows in sapphire substrate, AlGaInP (Aluminium Gallium Indium Phosphide, abbreviation AlGaInP) grows in GaAs (Gallium Arsenide is called for short GaAs) base material.Epitaxy technology can be applicable to the electromagnetic wave transmitting-receiving film of the transistor of manufacturing integration circuit, micro electronmechanical sensing element, communication element, the vibrating membrane that trap signal is used, the luminescent layer of light-emitting diode etc. or for detection of DNA (deoxyribonucleic acid) (Deoxyribonucleic acid is called for short DNA), antibody or amino acid whose chip etc.
But general gas production phase epitaxy method (the Vapor phase epitaxy of epitaxy technique again, be called for short VPE), molecular beam epitaxy (Molecular beam epitaxy, be called for short MBE) or liquid phase epitaxial method (Liquid phase epitaxy, be called for short LPE) etc., with vapour phase epitaxy method, industry is used metal organic chemical vapor deposition (Metal organic chemical vapor deposition mostly at present, be called for short MOCVD) or hydride gas-phase epitaxy (Hydride vapor phase epitaxy, be called for short HVPE), correlation technique can be joined Japanese patent of invention and be disclosed JP No. 2010135598, U.S.'s patent of invention discloses US No. 2006/0115933, U.S.'s patent of invention discloses US No. 2010/0221902, U.S.'s patent of invention discloses US No. 2007/0224786, U.S.'s patent of invention discloses US2010/0006024 number, U.S.'s patent of invention discloses US No. 2011/0012109, U.S.'s patent of invention is announced US 7,943, No. 492, U.S.'s patent of invention is announced US 7,883, No. 996 and U.S.'s patent of invention are announced US 7,427, No. 555 etc.
The principle of epitaxial film growth is atom with the lattice of base material as template and elongation growth, and then forms the film of mono-crystalline structures.But the epitaxial film that obtains with epitaxy technique still can produce fault in material unavoidably, comprises that hole (Voids), dislocation (Dislocations), tomography (Faults) are even field trash (Inclusions) etc.For the growth of homoepitaxy, the formation of defective may be to stem from base material itself more defective is namely arranged; The chemical composition of base material part is inhomogeneous; Processing chamber or gas source contain impurity; Perhaps deposition velocity is too fast, causes the atomic arrangement of epitaxial film to make a mistake.In the growth of heteroepitaxy, except aforementioned factor, also can owing to the atomic size between epitaxial film and base material and lattice direction difference, the defect concentration of epitaxial film be increased.Furthermore, when atomic deposition during in the unsettled position of substrate surface, its energy is higher, if the temperature of deposition is not high enough, causes the mobile difficulty of atom, just causes easily the generation of defective.
With vapour phase epitaxy method, owing to belong to non-equilibrium growth, so post-depositional atom just was difficult to move at substrate surface originally, the atom that is deposited on dislocation place is gasified and redeposited, therefore, defect concentration will significantly increase.On the contrary, if epitaxy technique can be near balanced growth, namely the interface atom of liquid-solid phase can deposit and melting simultaneously, and then the defect concentration of epitaxial film can be lower.Take the epitaxial film of blue light-emitting diode as example, often by vapour deposition process gallium nitride is grown up in sapphire substrate, wherein, the stable phase of gallium nitride is the buergerite (Wurtzite) of hexagonal crystal system, and sapphire is hexagonal crystal system (0002) face, that is to say, the lattice between gallium nitride and the sapphire does not mate (Lattice mismatch) will be above 13%, when using from sapphire substrate that the liquid phase condensate crystallization obtains, its dislocation density will be up to 10
9/ cm
2By contrast, the silicon wafer dislocation density of pulling out crystal bar in liquation only has 10
4/ cm
2
Dislocation density in the epitaxial film is higher, and the character of its wafer is just poorer.The explanation as an example of integrated circuit example, the increase of dislocation density can affect the reduction of current signal and noise is increased.Again take light-emitting diode as example, the generation of dislocation can reduce the photon numbers that is produced by internal quantum efficiency (Internal quantum effect), and when temperature raises, the size of dislocation can strengthen and cause irreversible luminosity to decay, again with gallium nitride/sapphire extension, the average headway of its dislocation is about 1 μ m only, will scattering occur and produce heat energy if photon runs into dislocation between advancing.Hence one can see that, reduces defect concentration and can improve the brightness of light-emitting diode, and prolong its useful life.
For solving the defect problem of above-mentioned epitaxial film, generally adopt annealing (Annealing) technique, epitaxial film is heated to high temperature, atom in it can be spread and rearrange; Or bring out by this movement of dislocation, make it eliminate each other (offseting towards the relative direction slippage such as positive dislocation and negative dislocation), to reduce internal stress and defect concentration.This kind prior art is found in U.S.'s patent of invention and discloses US2007/0134901 number, U.S.'s patent of invention and disclose No. 2009/0050929, US and U.S.'s patent of invention and disclose No. 2010/0178749, US etc.Wherein, U.S.'s patent of invention discloses US2007/0134901 number and has disclosed a kind of method of building growth gallium arsenide epitaxy on the wafer at SiGe, silicon wafer is provided first, utilize high vacuum chemical vapour deposition (Ultra-high vacuum chemical vapordeposition, be called for short UHVCV) the grow up silicon germanium extension layer of a plurality of high Ge contents of system, then again with Metalorganic Chemical Vapor Deposition, in the surface of this silicon germanium extension layer growth gallium arsenide epitaxial layer, wherein, each individual layer must carry out in real time (in-situ) high annealing, carry out 0.25 to 1 hour annealing 750 ℃ temperature, atmosphere can be hydrogen, improves by this quality of germanium film extension.And U.S.'s patent of invention discloses US and has disclosed a kind of semiconductor substrate and manufacture method thereof that adopts for semiconductor optoelectronic element for No. 2009/0050929 outward, use atomic layer chemical vapor deposition (Atomic layer CVD, be called for short ALCVD) at substrate surface growth nitride resilient coating, after this nitride resilient coating forms, this nitride resilient coating can further carry out annealing in process in the temperature between 400 ℃ to 1,200 ℃.U.S.'s patent of invention discloses US and has disclosed a kind of method of making the epitaxial growth floor at compound for No. 2010/0178749 again, with extensional mode at least one material layer is grown up on composite structure first, this composite structure comprises support base material, be incorporated into the film of this support base material and by Low Pressure Chemical Vapor Deposition (Low pressure chemical vapor deposition, abbreviation LPCVD) is formed at the binder course between this support base material and this film, this binder course is the faying face that is formed at this support base material, a faying face or both silica of this film, behind this material layer to be formed, heat-treat being higher than the temperature that deposits this oxide skin(coating), this heat treatment is for remaining on the scheduled time.
Though above-mentioned technique can reduce defect concentration, because the temperature gradient that annealing produces makes epitaxial film break easily; And, because the internal stress of epitaxial film is unbalanced, so when temperature raise, the lattice of epitaxial film can soften and produce distortion; The more important thing is that general annealing process is limited to the amplitude of the defect concentration decline of epitaxial film, namely can't effectively improve the defect concentration of epitaxial film.
Summary of the invention
Main purpose of the present invention is to solve the problem that existing annealing process can't further reduce the defect concentration of epitaxial film.
For reaching above-mentioned purpose, the invention provides a kind of method for annealing that reduces the defective of epitaxial film, it is characterized in that the epitaxial film of being grown up by gas-phase deposition on base material is imposed between 10MPa to 6, pressure between the 000MPa, and heat this epitaxial film to the temperature of the fusing point that is lower than this epitaxial film and remain on annealing time greater than 1 minute.
In one embodiment of the invention, this gas-phase deposition is metal organic chemical compound vapor deposition technique.
In one embodiment of the invention, this pressure is to use transmission medium to put on this epitaxial film, and this transmission medium is to be selected from the group that is comprised of graphite powder, hexagonal crystal system boron nitride powder, molybdenum disulphide powder, talcum powder, pyrophyllite powder, pulverized limestone, dolomite dust and salt.
In one embodiment of the invention, this pressure is to utilize isostatic pressing or single shaft pressurization to put on this epitaxial film.
In one embodiment of the invention, this base material is to be selected from the group that is comprised of sapphire, carborundum, gallium nitride and silicon.
In one embodiment of the invention, this epitaxial film is gallium nitride or silicon.
In one embodiment of the invention, this base material has the thickness between 420 μ m to 440 μ m.
In one embodiment of the invention, this epitaxial film has the thickness between 2 μ m to 7 μ m.
In one embodiment of the invention, this epitaxial film is in atmosphere, and this atmosphere is selected from by the argon-mixed group that forms of nitrogen, nitrogen and hydrogen mixture, argon gas, argon hydrogen gaseous mixture and nitrogen.
In one embodiment of the invention, this epitaxial film is in oscillation environment.
In one embodiment of the invention, this annealing time is between 5 minutes to 10 hours.
For reaching above-mentioned purpose, the present invention also provides a kind of epitaxial film with fabricating low-defect-density, to grow up in base material with gas-phase deposition, it is characterized in that this epitaxial film through being heated to the fusing point that is lower than this epitaxial film temperature and stand between 10MPa to 6 pressure between the 000MPa.
In one embodiment of the invention, this gas-phase deposition is metal organic chemical compound vapor deposition technique.
In one embodiment of the invention, this pressure utilizes isostatic pressing or single shaft pressurization to put on this epitaxial film.
In one embodiment of the invention, this base material is selected from the group that is comprised of sapphire, carborundum, gallium nitride and silicon.
In one embodiment of the invention, this epitaxial film is gallium nitride or silicon.
In one embodiment of the invention, this base material has the thickness between 420 μ m to 440 μ m.
In one embodiment of the invention, this epitaxial film has the thickness between 2 μ m to 7 μ m.
In one embodiment of the invention, this pressure is to use transmission medium to put on this epitaxial film, and this transmission medium is selected from the group that is comprised of graphite powder, hexagonal crystal system boron nitride powder, molybdenum disulphide powder, talcum powder, pyrophyllite powder, pulverized limestone, dolomite dust and salt.
As known from the above, the present invention reduce the method for annealing of epitaxial film defective and the epitaxial film that obtains with the method compared with prior art accessible beneficial effect be:
One, the present invention can and then alleviate the crystal lattice stress of this epitaxial film by this epitaxial film is applied this pressure, so that the defect concentration of this epitaxial film significantly reduces;
Two, simultaneously, this pressure also can promote the movement of atom in this epitaxial film, makes it can move to easilier stable lattice position under this temperature, with the quantity of reduce injection defect.
Three, when selecting to use this isostatic pressing, when this epitaxial film stood this pressure, the pressure differential of all directions can appropriateness be offset, and in the situation of not destroying this epitaxial film, is applied to this epitaxial film with this higher pressure thus, reaches better defect concentration.
Description of drawings
Figure 1A to Fig. 1 D is the manufacturing process schematic diagram of one embodiment of the present of invention.
Fig. 2 A to Fig. 2 D is the manufacturing process schematic diagram of another embodiment of the present invention.
Fig. 3 is the Process configuration schematic diagram of further embodiment of this invention.
Fig. 4 is the pressure-temperature phasor of gallium nitride.
Embodiment
The present invention relates to a kind of method for annealing that reduces the defective of epitaxial film, and the epitaxial film that uses this method for annealing to obtain, please consult first Figure 1A to Fig. 1 D, manufacturing process schematic diagram for one embodiment of the invention, shown in Figure 1A, base material 10 is provided first, in the present embodiment, this base material 10 has the thickness between 420 μ m to 440 μ m, this base material 10 is sapphire (being alumina single crystal), be the plate shape substrates that obtains from the cutting of sapphire crystal bar, the upper surface 11 of this base material 10 is (0001) lattice plane (also claiming C-plane) of aluminium oxide, but the present invention is not limited to (0001) lattice plane with aluminium oxide as this upper surface 11, according to practical application, also can select (1-102-) lattice plane (also claiming R-Plane) or (0001) lattice plane (also claiming M-Plane) as this upper surface 11.In addition, in the present embodiment, this sapphire crystal bar can be by Chai Shi (czochralski method, Czochralski, abbreviation CZ) method, the laminar crystal growth in limit limit (Edge-defined film-fed growth is called for short EFG) method, vertical-horizontal temperature gradient cooling (Vertical horizontal gradient freezing, being called for short VHGF) (kyropoulos method, Kyropoulos) method etc. makes for method, Kai Shi.
See also Figure 1B, after the preparation of finishing this base material 10, utilize gas-phase deposition growing epitaxial film 20 on this base material 10, this epitaxial film 20 has the thickness between 2 μ m to 7 μ m, this epitaxial film 20 of present embodiment is gallium nitride, and this gas-phase deposition is preferably the organic chemical vapor deposition method of using, it carries out using the organic chemical vapor deposition system, for example by Aixtron, the organic chemical vapor deposition system of the manufacturers produce such as Veeco or Sanso, this system roughly comprises reaction chamber, vacuum pump, heater, gas supply unit and gas control unit, this heater is located in this reaction chamber, this vacuum pump is connected to this reaction chamber, this gas supply unit comprises the first gas source, the second gas source and current-carrying gas source, this first gas source, this second gas source and this current-carrying gas source respectively via pipeline connection to this reaction chamber, this gas control unit is controlled the gas flow of this pipeline, adjusts by this air pressure of this reaction chamber.
Illustrate with the cvd nitride gallium, first this base material 10 is positioned in this reaction chamber, extract this reaction chamber to the certain vacuum degree with this vacuum pump.If this epitaxial film 20 is gallium nitride, this first gas source should be selected trimethyl gallium (Trimethylgallium is called for short TMG) or (Triethylgallium is called for short TEG), and this second gas source should be selected ammonia (NH
3), and hydrogen (H should be used in this current-carrying gas source
2) or nitrogen (N
2).Then, make with this heater and to be increased to 500 ℃ and 1 in this reaction chamber, temperature between 000 ℃, and the gas in this first gas source, this second gas source and this current-carrying gas source mixed pass into this reaction chamber, chemical reaction by this reaction intracavity gas, gallium nitride is grown at the upper surface 11 of this base material 10, finally obtain being formed at this epitaxial film 20 of this base material 10.Above-mentioned only with the cvd nitride gallium as an example, the present invention does not limit this employed technological parameter of organic chemical vapor deposition system and reactant, form the materials demand of this epitaxial film 20 according to institute's wish, this first gas source also can be trimethyl indium (Trimethylindium, abbreviation TMI), triethylindium (Triethylindium, abbreviation TEI), zinc methide (Dimethylzinc, be called for short DMZ) etc., this second gas source also can be arsenic hydride, and (Arsine is called for short AsH
3), (Phosphine is called for short PH to hydrogen phosphide
3) etc.
As shown in Figure 1B, this epitaxial film 20 has a plurality of defectives 21, with gallium nitride, do not pass through any heat treatment before, the density of this defective 21 is about 10
8/ cm
2To 10
9/ cm
2Generally speaking, monocrystalline intracrystalline " defective " should be contained point defect (Point defects), line defect (Line defects), planar defect (Planar defects) and volume defect (Bulk defects), wherein, point defect comprises vacancy defect (Vacancy defects), interstitial defect (Interstitial defects) or impurity (Impurities) etc., line defect comprises edge dislocation (Edge dislocation), screw dislocation (Screw dislocation) etc., planar defect comprises the stacking fault (Stacking fault) of atom, volume defect then comprises hole (Voids) or precipitate (Precipitates), but alleged " defective " mainly refers to line defect (being edge dislocation and screw dislocation) among the present invention, planar defect and volume defect.
Please continue to consult Fig. 1 C, after the deposition of finishing this epitaxial film 20, this epitaxial film 20 be carried out annealing in process, (Meltingtemperature is called for short T this epitaxial film 20 being heated to the fusing point that is lower than this epitaxial film
m) temperature the time, also this epitaxial film 20 is applied between 10MPa to 6, the pressure between the 000MPa, this annealing in process can use high-temperature atmosphere furnace, spark plasma sintering (Spark plasma sintering is called for short SPS) stove or heat all to press stove.Present embodiment such as the high-temperature atmosphere furnace of being produced by Lindberg, is put into this high-temperature atmosphere furnace with this base material 10 together with this epitaxial film 20 to use this high-temperature atmosphere furnace as an illustration first.This base material 10 is to be coated by transmission medium 30 with this epitaxial film 20, this transmission medium 30 can be graphite powder, the hexagonal crystal system boron nitride powder, molybdenum disulphide powder, talcum powder, pyrophyllite powder, pulverized limestone, dolomite dust, the mixture of salt or previous materials, because previous materials all is Powdered under normality, for ease of arranging, this transmission medium 30 is preferably colded pressing (Cold compression) through mould first or hot pressing (Hot pressing) has the fixedly base substrate of body with formation, the material of this mould can be steel alloy, tungsten carbide, graphite or other and previous materials have metal and the pottery of similar characteristics, in addition, at least a pressure-applying unit 40 of pressure to this transmission medium 30 that provide also need be set in this high-temperature atmosphere furnace, for guaranteeing evenly to apply pressure to this epitaxial film 20, this pressure-applying unit 40 is preferably and is symmetrical arranged.
Shown in Fig. 1 C, in the present embodiment, the quantity of this pressure-applying unit 40 is six, only illustrate four among the figure, namely this pressure-applying unit 40 comprises the first presser unit 41, the second presser unit 42, the 3rd presser unit 43, the 4th presser unit 44, this first presser unit 41 and this second presser unit 42 are arranged at respectively top and the below of this epitaxial film 20, the 3rd presser unit 43 and the 4th presser unit 44 are arranged at respectively left side and the right side of this epitaxial film 20, in addition, this pressure-applying unit 40 comprises that also the slender acanthopanax at the place ahead of being located at respectively this epitaxial film 20 and rear presses unit and the 6th presser unit, present embodiment is only take the quantity of this pressure-applying unit 40 as six as an example explanations, but the present invention is not limited to this, the quantity of this pressure-applying unit 40 and set-up mode should with provide this epitaxial film 20 each to the pressure of equalization as considering.In addition, above-described embodiment is exerted pressure as example by 30 pairs of these base materials of this transmission medium 10 and this epitaxial film 20 with this pressure-applying unit 40, but the present invention is not limited to this, and according to the actual requirements, this pressure-applying unit 40 also can directly apply pressure to this base material 10 and this epitaxial film 20.And, the present invention's definition is between 10MPa to 6, this pressure between the 000MPa refers to the force value that this epitaxial film 20 is subject to, and these pressure-applying unit 40 actual pressure that should export should be looked whether this transmission medium 30 arranges, the factors such as design of the material of this transmission medium 30 and disposing way and this pressure-applying unit 40 determine.
To be placed in this high-temperature atmosphere furnace, namely heat this base material 10 and this epitaxial film 20 to this temperature, and be incubated an annealing time, simultaneously, apply this pressure by this pressure assembly 40 by 30 pairs of these epitaxial films 20 of this transmission medium, wherein, this base material 10 passes into gas in this high-temperature atmosphere furnace so that can be in an atmosphere with this epitaxial film 20, this atmosphere can be nitrogen, nitrogen and hydrogen mixture, argon gas, argon hydrogen gaseous mixture or nitrogen are argon-mixed, through behind this annealing time, make this high-temperature atmosphere furnace and this interior pressure assembly 40 thereof be down to room temperature and normal pressure, the quantity of this defective 21 in this epitaxial film 20 that obtains is minimized, shown in Fig. 1 D.In the present invention, this temperature should be selected according to the material behavior of this epitaxial film 20, and wherein, this temperature is preferably between 0.3T
mTo 0.9T
mBetween.If the gallium nitride that uses with present embodiment is as example, its fusing point (or sublimation point) can change with the difference of pressure, as shown in Figure 4, pressure-temperature phasor for gallium nitride, if putting on this pressure of this epitaxial film 20 is between 10MPa to 6, between the 000MPa, this temperature should be chosen as between 400 ℃ to 2,250 ℃, in addition, this annealing time should be greater than 1 minute, can between 5 minutes to 10 hours, be preferably between 1 hour to 8 hours, accordingly, via this epitaxial film 20 that this annealing in process obtains, the density of this defective 21 can be from 10
8/ cm
2To 10
9/ cm
2Between be reduced to 10
4/ cm
2To 10
6/ cm
2Between.Except making this base material 10 and this epitaxial film 20 this temperature continues one section this annealing time, the present invention also can make this base material 10 be heated to this temperature with this epitaxial film 20 at this annealing time of multistage, and every section this annealing time is shorter, for example: first this base material 10 is heated to this temperature with this epitaxial film 20, be incubated and be down to room temperature after 30 minutes, after room temperature keeps 30 minutes, be warming up to again this temperature, and carry out this annealing in process according to this.
Please continue to consult Fig. 2 A to Fig. 2 D, be the manufacturing process schematic diagram of another embodiment of the present invention, Figure 1A, Figure 1B and Fig. 1 D of Fig. 2 A, Fig. 2 B and the similar above-described embodiment of Fig. 2 D be not so give unnecessary details separately.But compare with above-described embodiment, present embodiment adopts the single shaft pressurization, see also Fig. 2 C, wherein, this pressure-applying unit 40 only is made of with this second presser unit 42 this first presser unit 41, be located at respectively top and the below of this epitaxial film 20, use provide these epitaxial film 20 single shafts to stress.Other sees also Fig. 3, Process configuration schematic diagram for further embodiment of this invention, the present invention also is applicable to simultaneously a plurality of these base materials 10,10a is stacking anneals, and at a plurality of these base materials 10,10a grow up respectively this epitaxial film 20,20a, this epitaxial film 20a also comprises a plurality of defectives 21 first.Subsequently, growth there is this epitaxial film 20, this base material 10 of 20a, the 10a vertical stacking, again with this single shaft pressurization to this stacked base material 10,10a and this epitaxial film 20,20a exerts pressure and carries out this annealing in process, wherein, for this epitaxial film 20 is provided, the more uniform stress of 20a, and avoid this base material 10a or this epitaxial film 20a broken by these base material 10 direct pressurizeds of top, present embodiment preferably arranges resilient coating 50 between this base material 10 and this epitaxial film 20b, this resilient coating 50 can be graphite paper, the nonwoven fabrics that is made by graphite fibre, by weaving cotton cloth of obtaining of graphite fibre braiding or flexible material that other form with graphite, because the setting of this resilient coating 50, so that can directly not contact between this base material 10 this epitaxial film 20a, avoid this base material 10a or this epitaxial film 20a under the environment of high pressure and high temperature, to produce distortion even break.
In addition, the present invention also can in to this epitaxial film 20 pressurized, heated the time, utilize the concussion source that this epitaxial film 20 is shaken; Perhaps, by this pressure assembly and this transmission medium 30 this epitaxial film 20 is shaken.This concussion source can be the ultrasonic vibrating device, and should can be fixed in the high temperature furnace equipment of this base material 10 of heating and this epitaxial film 20 in the concussion source, wherein, the amplitude in this concussion source and frequency should be selected according to the material behavior of this epitaxial film 20, take this epitaxial film 20 of above-described embodiment as gallium nitride as an example, the amplitude in this concussion source is preferably between 10 μ m to 30 μ m, and calibration ground is between between the 20kHz to 40kHz.By assisting of concussion, can further accelerate the movement of this defective 21, so, can the density of this defective 21 be dropped to a certain degree in short time or lower temperature.
Above-described embodiment comprises that for using gallium nitride and sapphire light-emitting diode illustrate as an example, but the field of the invention should contain any element that relates to epitaxy technology makes, and for example is applied to the light-emitting diode of other chemical compositions or structure, the manufacturing of integrated circuit or the technique of solar cell.
The present invention mainly is when carrying out this annealing in process, simultaneously this epitaxial film is applied this pressure, alleviate thus the crystal lattice stress of this epitaxial film, and promote the movement of atom in this epitaxial film, to move to stable lattice position, compare with existing only epitaxial film the heating, do not apply the annealing in process of extra pressure, the present invention can make the defect concentration of this epitaxial film more reduce, and therefore, the quality of finishing this epitaxial film after this annealing in process will be more good.Secondly, by using this isostatic pressing, when making this epitaxial film be subjected to this pressure, the pressure differential of all directions can appropriateness be offset, so can improve this pressure that puts on this epitaxial film, and correspondingly alleviate the stress that atom is subject in this epitaxial film, so can accelerate the elimination of this defective, reach better defect concentration.Moreover the present invention this concussion source of can further arranging in pairs or groups makes this epitaxial film produce concussion, accelerates the movement of atom in this epitaxial film.
Below the present invention is had been described in detail, but above said content only is the preferred embodiments of the present invention that it can not limit scope of the invention process.The equivalent variations that claim is done according to the present invention and modification etc. all should comprise within the scope of the invention.
Claims (20)
1. method for annealing that reduces the epitaxial film defective, it is characterized in that, the epitaxial film of being grown up on base material by gas-phase deposition is imposed between 10MPa to 6, the pressure between the 000MPa, and heat described epitaxial film to the temperature of the fusing point that is lower than described epitaxial film.
2. the method for annealing of reduction epitaxial film defective according to claim 1 is characterized in that, described gas-phase deposition is metal organic chemical compound vapor deposition technique.
3. the method for annealing of reduction epitaxial film defective according to claim 1 is characterized in that, described pressure utilizes isostatic pressing or single shaft pressurization to put on described epitaxial film.
4. the method for annealing of reduction epitaxial film defective according to claim 1 is characterized in that, described base material is selected from the group that is comprised of sapphire, carborundum, gallium nitride and silicon.
5. the method for annealing of reduction epitaxial film defective according to claim 1 is characterized in that, described epitaxial film is gallium nitride or silicon.
6. the method for annealing of reduction epitaxial film defective according to claim 1 is characterized in that, described base material has the thickness between 420 μ m to 440 μ m.
7. the method for annealing of reduction epitaxial film defective according to claim 1 is characterized in that, described epitaxial film has the thickness between 2 μ m to 7 μ m.
8. the method for annealing of reduction epitaxial film defective according to claim 1, it is characterized in that, described pressure uses transmission medium to put on described epitaxial film, and described transmission medium is selected from the group that is comprised of graphite powder, hexagonal crystal system boron nitride powder, molybdenum disulphide powder, talcum powder, pyrophyllite powder, pulverized limestone, dolomite dust and salt.
9. the method for annealing of reduction epitaxial film defective according to claim 1, it is characterized in that, described epitaxial film is in atmosphere, and described atmosphere is selected from by the argon-mixed group that forms of nitrogen, nitrogen and hydrogen mixture, argon gas, argon hydrogen gaseous mixture and nitrogen.
10. the method for annealing of reduction epitaxial film defective according to claim 1 is characterized in that, described epitaxial film is in oscillation environment.
11. the method for annealing of reduction epitaxial film defective according to claim 1 is characterized in that, described epitaxial film is at the annealing time of described temperature maintenance greater than 1 minute.
12. the method for annealing of reduction epitaxial film defective according to claim 11 is characterized in that described annealing time is between 5 minutes to 10 hours.
13. epitaxial film with fabricating low-defect-density, it is grown up on base material with gas-phase deposition, it is characterized in that, described epitaxial film is through annealing in process, described annealing in process is that the described epitaxial film of heating applies between 10MPa to 6 pressure between the 000MPa to the temperature of the fusing point that is lower than described epitaxial film and to described epitaxial film.
14. the epitaxial film with fabricating low-defect-density according to claim 13 is characterized in that, described gas-phase deposition is metal organic chemical compound vapor deposition technique.
15. the epitaxial film with fabricating low-defect-density according to claim 13 is characterized in that, described pressure utilizes isostatic pressing or single shaft pressurization to put on described epitaxial film.
16. the epitaxial film with fabricating low-defect-density according to claim 13 is characterized in that described base material is selected from the group that is comprised of sapphire, carborundum, gallium nitride and silicon.
17. the epitaxial film with fabricating low-defect-density according to claim 13 is characterized in that, described epitaxial film is gallium nitride or silicon.
18. the epitaxial film with fabricating low-defect-density according to claim 13 is characterized in that, described base material has the thickness between 420 μ m to 440 μ m.
19. the epitaxial film with fabricating low-defect-density according to claim 13 is characterized in that, described epitaxial film has the thickness between 2 μ m to 7 μ m.
20. the epitaxial film with fabricating low-defect-density according to claim 13, it is characterized in that, described pressure is to use transmission medium to put on described epitaxial film, and described transmission medium is selected from the group that is comprised of graphite powder, hexagonal crystal system boron nitride powder, molybdenum disulphide powder, talcum powder, pyrophyllite powder, pulverized limestone, dolomite dust and salt.
Applications Claiming Priority (2)
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|---|---|---|---|
| TW100131006A TW201310537A (en) | 2011-08-30 | 2011-08-30 | Annealing method of reducing the epitaxial film defect and epitaxial film made by the method |
| TW100131006 | 2011-08-30 |
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| CN102969241A true CN102969241A (en) | 2013-03-13 |
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| Country | Link |
|---|---|
| US (1) | US20130052838A1 (en) |
| KR (1) | KR20130024709A (en) |
| CN (1) | CN102969241A (en) |
| TW (1) | TW201310537A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103578977A (en) * | 2013-11-19 | 2014-02-12 | 中国科学院半导体研究所 | Method for improving fluorescence intensity of AlN epitaxial thin film |
| CN112071748A (en) * | 2020-09-18 | 2020-12-11 | 松山湖材料实验室 | Preparation method of low-point defect density wide-bandgap semiconductor single crystal epitaxial film |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150206765A1 (en) * | 2014-01-17 | 2015-07-23 | Sandia Corporation | Mechanical Compression-Based Method for the Reduction of Defects in Semiconductors |
| CN110499530B (en) * | 2019-08-28 | 2023-09-12 | 大同新成新材料股份有限公司 | Production equipment and method for electronic silicon carbide chip |
| CN111807315B (en) * | 2020-07-20 | 2023-10-03 | 中国科学院长春光学精密机械与物理研究所 | Conductive oxide plasmon nanometer optical antenna and preparation method thereof |
| CN115058700B (en) * | 2022-06-24 | 2023-07-07 | 电子科技大学中山学院 | Preparation method of molybdenum disulfide film and molybdenum disulfide film |
| CN116867347B (en) * | 2023-09-01 | 2023-12-19 | 北京中博芯半导体科技有限公司 | Method for adjusting AlN heteroepitaxial surface internal stress |
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2011
- 2011-08-30 TW TW100131006A patent/TW201310537A/en unknown
- 2011-11-01 CN CN2011103405129A patent/CN102969241A/en active Pending
- 2011-12-23 US US13/336,757 patent/US20130052838A1/en not_active Abandoned
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- 2012-02-08 KR KR1020120012857A patent/KR20130024709A/en not_active Application Discontinuation
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| CN1480569A (en) * | 2002-06-27 | 2004-03-10 | ͨ�õ�����˾ | Method of reducing crystal defect density |
| CN101724910A (en) * | 2009-12-02 | 2010-06-09 | 南京大学 | Method for eliminating surface defects of GaN thick film material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103578977A (en) * | 2013-11-19 | 2014-02-12 | 中国科学院半导体研究所 | Method for improving fluorescence intensity of AlN epitaxial thin film |
| CN103578977B (en) * | 2013-11-19 | 2016-08-24 | 中国科学院半导体研究所 | The method improving fluorescence intensity of AlN epitaxial thin film |
| CN112071748A (en) * | 2020-09-18 | 2020-12-11 | 松山湖材料实验室 | Preparation method of low-point defect density wide-bandgap semiconductor single crystal epitaxial film |
| CN112071748B (en) * | 2020-09-18 | 2023-04-25 | 松山湖材料实验室 | Preparation method of low-point defect density wide-forbidden-band semiconductor single crystal epitaxial film |
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| US20130052838A1 (en) | 2013-02-28 |
| KR20130024709A (en) | 2013-03-08 |
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